Potassium Phosphate, Tribasic → HCID 54022783、化合物

HRID 1757067

反応式

HRID 1757067 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])=[CH:4][CH:3]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].[OH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1B(O)O.[Cl-].[Na+].C(OCC)(=O)C>C(COC)OC.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[OH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH3:12])=[O:10])=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 316783Methyl 2-(4-bromophenyl)acetateHCID 2773454(2-Hydroxyphenyl)boronic acidHCID 86643102Sodium chloride ethyl acetate

生成物 1

HCID 54022783HCID 54022783、化合物収率 75%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

Methyl (4-bromophenyl)acetate (2.79 g, 12.2 mmol), tetrakis(triphenylphosphine)palladium (0) (170 mg), potassium phosphate (9.71 g, 45.75 mmol) and dimethoxyethane (50 ml) were degassed under nitrogen in a 100 ml flask fitted with a reflux condenser. 2-Hydroxybenzene boronic acid (2.52 g, 18.3 mmol) in dimethoxyethane (5 ml) was added and the mixture was heated at reflux overnight then mixed with 1:1 saturated sodium chloride/ethyl acetate (25 ml). The organic materials were separated, dried (MgSO4), then concentrated under reduced pressure. The residue was purified by flash chromatography (SiO2, gradient hexane to 3:1 hexane/ethyl acetate) which provided 2.21 g (75%) of methyl (4-(2-hydroxyphenyl)phenyl)acetate.

後処理

  1. customfitted with a reflux condenser
  2. temperaturethe mixture was heated
  3. temperatureat reflux overnight
  4. customThe organic materials were separated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash chromatography (SiO2, gradient hexane to 3:1 hexane/ethyl acetate) which

出典と根拠

ORDレコード
ord-119d19062c6a4c3493b53a9fdf7b7d7b
出典データセット
uspto-grants-1995_08
特許番号
US05444050

関連ノート

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